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Laboratory Notebook
Two Patents describe a method for making the antihistamine drug Loratidine (Claritin)
- US sales of $2.7 billion
- the two patents are essentially identical
- Medichem sued to invalidate Rolabo patent and claimed priority
- Medichem had to prove it used the method to make loratidine before Rolabo did
A co-inventor’s lab notebook was a primary piece of evidence to support Medichem’s claim
- documented analysis of a sample claimed to be made using the patented method
- NMR spectral data confirmed the production of loratidine
The evidence was not enough to support Medichem's claim of reduction to practice
- NMR data do not show the process by which loratidine was made
- lab books were not witnessed
Rolabo Pharmaceuticals won the case (and the rights to make Loratidine)
because of problems with a Lab Notebook!!
Nature Reviews Drug Discovery (2006) 5, 180
Tools of the Trade
Weight Measurements
l1 l2
Double-pan balance
(a) balance beam suspended on a
sharp knife edge
(b) Standard weights are added to
m1 m2 the second pan to balance
sample weight
m m (c) Weight of sample is equal to the
total weight of standards
m1l1 = m2l2
Tools of the Trade
Weight Measurements
Single-pan balance
(a) balance beam suspended on a sharp knife edge
(b) Sample pan is balanced by counterweights on right
(c) Knob adjusted to remove weights from a bar above the pan
(d) Pan is moved back to its original position and the removed
weights equals the mass of the sample.
Tools of the Trade
Weight Measurements
Electronic balance
(a) Uses electromagnetic force to return the pan to original position
(b) Electric current required to generate the force is proportional to sample mass
(iii) Taring:
Done on many modern electronic balances
Container is set on balance before sample is added
Container’s weight is set automatically to read “0”
Tools of the Trade
Weight Measurements
1.) Burets
(i) Purpose: used to deliver multiple aliquots of a liquid in known volumes
Buret Smallest Tolerance (mL)
volume (ml) graduation (ml)
5 0.01 ± 0.01
10 0.05 or 0.02 ± 0.02
25 0.1 ± 0.03
50 0.1 ± 0.05
100 0.2 ± 0.10
Meniscus at 9.68 mL
Tools of the Trade
Volume Measurements
1.) Burets
(iii) always read the buret at the same eyelevel as the liquid
Avoids parallax errors
eyelevel View from above
15.46 mL 15.31 mL
1% error
(iv) Consistently read all levels versus a given position on the nearest mark
Tools of the Trade
Volume Measurements
1.) Burets
(v) Estimate the buret reading to the nearest 1/10 of a division
(vi) expel all air bubbles from the stopcock prior to use
(vii) rinse the buret with a solution 2-3x before filling the buret for a titration
(viii) Near the end of a titration, volume of 1 drop or less per delivery should be
used with the buret.
Tools of the Trade
Volume Measurements
stopper
Stopper the flask and mix solution by inversion (40 or more times)
(for later use) Remix by inverting the flask if the solution has been sitting
unused for more than several hours
Glass adsorbs trace amount of chemicalsclean using acid wash
- adhere to surface
Tools of the Trade
Volume Measurements
Pipet volume (mL) Accuracy (%) Precision (%) Accuracy (%) Precision (%)
Adjustable pipets
10 ±0.88 ±0.4
25 ±0.88 ±0.3
3.) Process:
(i) pour slurry of precipitate down a glass rod to
prevent splattering.
(ii) dislodge solid from beaker/rod with rubber
policeman
(iii) use wash liquid (squirt bottle) to transfer particles to
filter paper
(iv) dry sample
Rubber policeman
Tools of the Trade
Drying
3.) Dessicator: used to cool and store reagent or sample over long periods of
time.
(i) Contains a drying agent to absorb water from the atmosphere
(ii) Airtight seal
Experimental Error & Data Handling
Introduction
1.) Definition: The minimum number of digits needed to write a given value
(in scientific notation) without loss of accuracy.
(i) Examples:
(ii) occur at the end of number and to the right of the decimal point
3.) The last significant figure in any number is the first digit with any
uncertainty
(i) the minimum uncertainty is ± 1 unit in the last significant figure
(ii) if the uncertainty in the last significant figure is ≥ 10 units, then one less
significant figure should be used.
(iii) Example:
4.) Whenever taking a reading from an instrument, apparatus, graph, etc. always
estimate the result to the nearest tenth of a division
(i) avoids losing any significant figures in the reading process
7.45 cm
Experimental Error & Data Handling
Significant Figures
3.261 x 10-5
x 1.78
3 significant figures
5.80 x 10-5
34.60
) 2.4287
4 significant figures
14.05
Experimental Error & Data Handling
Significant Figures
a = 10b or Log(a) = b
(ii) example:
The logarithm of 100 is 2, since:
100 = 102
Log(339) = 2.530
character mantissa
Experimental Error & Data Handling
Significant Figures
(vi) Example:
(viii) Example:
8.) Graphs
(i) use graph paper with enough rulings to accurately graph the results
(ii) plan the graph coordinates so that the data is spread over as much of the
graph as possible
(iii) in reading graphs, estimate values to the nearest 1/10 of a division on the
graph
Experimental Error & Data Handling
Significant Figures
8.) Graphs
(ii) plan the graph coordinates so that the data is spread over as much of the
graph as possible
(iii) in reading graphs, estimate values to the nearest 1/10 of a division on the
graph
Experimental Error & Data Handling
Errors
True value
0.04
Re l . Uncert .(%) ( 100 ) 1.3% 1% 1 sig. fig.
3.06
Note: To avoid round-off error, keep one digit beyond the last
significant figure in all calculations.
- drop only when the final answer is obtained
Round-off errors
Experimental Error & Data Handling
Errors
Re l . Uncert .
0.03 ( 100 ), 0.02 ( 100 ) , 0.02 ( 100 )
1.76 1.89 0.59
Absolute Uncertaint y
Relative Uncertaint y(%) ( 100 )
Calculated Value
Rearrange:
4.0%
Absolute Uncertaint y ( 5.64 ) 0.23 0.2 1 sig. fig.
100
Experimental Error & Data Handling
Errors
(v) Example:
1.76 0.03 0.59 0.02 0.619 ? 3 sig. fig.
1.89 0.02
First operation: differences in brackets
Errors
3 sig. fig.
3.3% 3% 3.1% 1.1%
2 2
1 sig. fig.
Experimental Error & Data Handling
Errors
(vii) Example:
1.019 (±0.002)
Result & uncertainty match
in decimal place
28.42 (±0.05)
But:
12.532 (±0.064) too many significant figures
Errors
23.97
2.596966414
9.23
Experimental Error & Data Handling
Errors
Example
Find the absolute and percent relative uncertainty and express the answer with
a reasonable number of significant figures: